In order to analyze actinide elements in radioactive metal waste, the dissolution and chemical separation conditions were optimized. The surfaces of a type 304 stainless steel plate and of pipe waste sampled from the prototype advanced thermal reactor (Fugen) were dissolved in mixed acid solution (HNO(3):HCl:H(2)O = 1:1:4). The resulting solution was evaporated to dryness and dissolved with 2 mol/dm(3) of HNO(3) to prepare sample solutions. In order to analyze trivalent actinide elements in the sample solution containing a large amount of Fe(III) (> 0.1 g) using TRU resin, the effect of Fe(III) concentration on the recovery of Am(III) and reduction effect of Fe(III) to Fe(II) with ascorbic acid were studied. On the basis of results of this study, chemical separation scheme was constructed and Pu and Am in the sample solutions were separated. Thorium and U in the sample solutions were separated with UTEVA resin. High recoveries for all experimented elements were obtained from the analysis of spiked sample solutions, the effectiveness of the method was confirmed.